Particles sizes effect on the rheological properties of nickel doped

Chemistry and Materials Research www.iiste.org
ISSN 2224- 3224 (Print) ISSN 2225- 0956 (Online)
Vol.3 No.9, 2013
65
Particles sizes effect on the Rheological properties of Nickel doped
Barium Titanate of Nano particle in IPN-polymer matrix
S.Srivastava, K.R.Gota
Department of Material Science and Metallurgical Enginerring
Maulana Azad National Insitute of Technology
Bhopal 462051(M.P.) INDIA
Abstract
In this article,we have synthesizedcomposite material by dispersing variable amount of nanoparticles of nickel-
doped BaTiO3 nanoparticulate in IPN-polymer matrix.The chemical composition of the selected specimen is
represented by general formula Ba(Ti1-zXz)O3,where X is Ni and z=0.2 and it was prepared by sol-gel technique.
For the preparation of the polymer-matrix composite materials, Polyurethane (PU) as soft phase and PEMA as
hard phase were selected as matrix materials.The polymer-based composite was fabricated from casting method
by dispersing the nanoparticles in the IPN matrix along with coupling agent (vinyl triethoxysilane). The results
from the X-ray diffractogram show that the diameter of the particles which are doped with nickel in the
specimen lie in the range of 20-60nm. SEM analysis was used to investigate the morphology of the doped
BaTiO3 as well as polymer composite. From the SEM observation, the nanoparticles of doped BaTiO3 were
found to be homogeneously dispersed in the polymer matrix. The ratio of soft/hard phase actually modifies the
crosslinking density of the respective polymer in the matrix and also shows the better impact on the rheological
properties. In this paper, the effect of particle size of fine doped BaTiO3 powder on rheological properties of
doped BaTiO3/IPN-polymer composite are discussed along with the role of soft/hard phase matrix. Tensile
strength, elongation at a fracture of IPN composite, and UTS strength were evaluated by Instran testing machine
at room temperature at a crosshead speed of 5mm/min. Better dispersion and strong crossliking showed better
hardness and tensile strength
Key Words: IPN-polymer, Nanoparticle, Rheology, Crosslinking, Polymer Composite
Introduction
Owing to its extremely high dielectric constant associated with a series of ferroelectric phase
transitions, BaTiO3 is commercially used in multilayer ceramic capacitors (MLCCs).In ferroelectric materials,
the direction of spontaneous polarization (Ps) can be reoriented between two or more equilibrium symmetrical
states by the application of an appropriate electric field. [1]. Spontaneous polarization in a ferroelectric material
arises from non-centrosymmetric arrangement of ions in its unit cell. An electric dipole moment is produced by
the shift of positive ions in a direction opposite to that of negative ions. A ferroelectric crystal generally has
certain regions which exhibit uniform alignment of electric dipoles and the spontaneous polarization in such
regions may be different from one another. Such regions with uniform polarization are called ferroelectric
domains. The formation of ferroelectric domains is defined by a balance of electrostatic and strain energies with
domain-wall energy. As the poling induces ferroelectric-domain switching and increases polarization, it is
expected to increase average ferroelectric-domain size, which in turn should increase the residual strain in grains.
Hence, BaTiO3 is used in different applications such as dynamic random-access memory, piezoelectric
transducer, thermistor, and actuator.
In 2008, approximately 90% (by volume) of the capacitor market was dominated by the ceramic
capacitors [2]. In contrast, various types of polymer film capacitors are predominantly used in applications
requiring low dielectric absorption and loss factors over a wide temperature range [3]. An interesting result was
found in various types of interpenetrating polymer network. An interpenetrating polymer network (IPN) can be
defined as a mix of polymers in network form without any substantial quantities of crosslink, graft or block
junctions among the several polymer chains, where at least one polymer is polymerized and/or cross linked in the
immediate presence of the others [4-6]. Compared with simple mixed polymers, block polymers, and inarched
polymers, IPN is characterized with interspace topology structure. The IPN technique can be a very effective
method to improve the properties of existing polymer materials and to synthesize new ones with special
properties. The compatibility of the two component polymers in an IPN is an important criterion in determining
its physical properties. Nano-composite of the IPN polymer matrix is a special class of the materials formed by
dispersing one or more kind of the particles at an almost molecular level into the matrix. The size of the
dispersed phase particle in the polymer varies from the conventional level to the nanolevel. Organic-inorganic
hybrid as a new class of the composite provides many outstanding mechanical, thermal, optical, electromagnetic,

Vol.3 No.9, 2013
66
and biological properties. Interpenetrating networks are formed by swelling or polymerization of cross linked
polymer with a monomer and crosslinking with the latter to produce interlocked networks. Therefore, IPN shares
some of the advantages of both the polymer blends and network polymers. Epoxy resins (ERs) are widely used as
matrices of high-performance composite materials because of their stiffness, chemical resistance and high
temperature stability. However, they are inherently brittle [7]. Polyurethanes (PUs) are composed of flexible soft
segments and rigid hard segments. The variations in the compositions of the soft and hard segments impart PUs a
wide range of physical properties [8-10]. The blending of different sorts of materials produces composite
structures which combine different material properties, or may reveal novel properties not existing in the
constituent phases [11-13]. For example, oxidicperovskite materials have been employed as ceramic filler in
various polymers and the dielectric, piezoelectric and pyroelectric properties of the composites have been
investigated in relation to the filling factor and the dielectric properties of the inclusions[14].
In this research article, Ni+2
ions doped BaTiO3 nanoparticles was fabricated by sol-gel route. Polyvinyl
alcohol (PVA) was used to encapsulate the ferroelectric crystallites within its network. These were interspersed
by using the spin-on technique in the IPN which was formed by two different PU prepolymer and 2-
hydroxymethyl methacrylate. A series of IPNs were synthesized in a way having –NCO and –OH ratios in
1.2:1.0 in PU network. Alternation of the cross linking density of the PU network was achieved by varying the
equivalent ratio of a tri-olto di-ol.
2. Experimental
2.1 Preparation of Ni-doped BaTiO3 by sol-gel methods
The compositions of the specimens can be represented by a general formula(BaTi1-zXz)O3, where X represents
the various substituted group, but in this case X is only Ni with z=0.3. The specimens of the dielectric materials
were prepared by sol-gel technique. The polymer template in Ba+2
and Ni in doped Ti+4
cations was arranged by
using PVA molecules and it was obtained by mixing barium acetate, titanium isopropoxide (TTIP, 97 %,
supplied by Aldrich Chemical), 15cc Isopropanol (99 %, supplied by Merck) and Ni(NO)3 was added drop by
drop into the prepared PVA solution. The required amount of ethyl alcohol and acetic acid in the volume ratio of
75:25 were prepared and the weighed amount of titanium isopropoxide, with Isopropanol was hydrolyzed with
proper stirring for 2 hours. Aqueous solution of barium acetate was poured into the mixture and the resulting
solution was stirred again for two hours. The solution was clear and transparent. In this mixture, aqueous
solution of Nickel nitrate was added drop by drop. In addition, PVA (3g/l) was added to this solution drop-wise
in 5:2 ratios. It was observed that at room temperature, several processes like hydrolysis and condensation
occurred in the resulting solution which eventually converted into gel. The gel was dried (in oven at 70o
C for
24hr) and then calcined at 750o
C to obtain the BaTiO3 phase.
2.2 Material and methods for the preparation of polymer network
All the raw material used in the preparation of the IPN network is commercially available in the market. The
crossed linked polyurethane components PUR, consisted of 1, 1’, 3, 3’-tetramethylxylene di-isocyanate
(TMXDI), ether type polyols(PPG1000 and PTMG 1000), 1,1,1- trimethyol propane (TMP), was stirred and
degassed in a flask at 70o
C under reduced pressure for 16 hours. Two major tasks involved in the preparation of
the IPN network are as follows (1) Preparation of HPU pre-polymer and (2) Crosslinking with HUP with PU in
1:1 ratio. The purified chemical along with 1, 1, 1 - trimethyl propane and 1, 4-butanediol was poured into 4-
necked reaction vessels and stirred where the reaction was carried out at room temperature. During the mixing
the mixture was flashed with nitrogen to remove the dissolve oxygen inside the mixture. It was again left for 24
hrs at 70o
C for further reaction and vaporization of the excess solvent from the mixture. Figure 1 depicts the
synthetic processes for the production of IPN polymer of PU and HPU pre-polymer.
2.3 Preparations of the compositematerials
The ferroelectric material was mixed with reactive polymer chain at 80o
C for 10 min. The mixture was poured
into a steel mold where the polymerization reaction took place. To avoid the settlement of the ferroelectric
materials inside the mixture, the mold vessels were made to continuously rotate on their axes with slightly
vibration. The steel mold was clamped with nitrile rubber of 8mm diameter which was placed in between the
steel clamps. The polymerization reaction along with the formation of composite materials occurred in three
different temperature which were 65, 85, and 95o
C. The volatile monomer and bubbles in the samples were
removed at low temperature. The composite powder samples were then hot pressed at 120◦C for 10 min under a
pressure of 130 MPa in a steel die of diameter 12 mm. The die was cooled to room temperature underthe
application of pressure.

Vol.3 No.9, 2013
67
2.4 Characterizations
Tensile testing requires hardened ‘dog-bone’ shaped samples created from the mixture which is
described above. The biggest challenge in creating the sample was to remove all the solvent and to ensure no air
pockets existed in the neck region of the sample. Multiple samples were created for each system. The mechanical
properties of ferroelectric material reinforced polymer composites, in the form of 25 mm x 9 mm x 0.7 mm test
samples, were measured at room temperature using an electro-mechanical testing machine (INSTRON-1195)
incorporating a tension/compression transducer (load cell) operated at constant strain rate.Tensile testing of all
the polymer composite was performed by application of stress on the material alongwith .Percentage elongation
and reductions in the area were computed.Isothermal testing conditions along with the temperature set up were
ensured to also study the temperature induced effects. At least five specimens were tested to obtain the averaged
values of the results. In order to evaluate the effect of filler content on the mechanical properties of ceramic
filled IPN polymer matrix, mechanical properties were also evaluated from the usual condition.
3. Results and discussion
3.1. Characterization of the Ferroelectric material
BaTiO3 is a basic ferroelectric material and having vast applications in different fields. It has two substituting
sites: one being Ba+2
sites and other from Ti+4
sites.According to the results observed by us, 30% of Ti+4
ions
are replaced by Ni+2
sites. The particles of three different sizes were prepared from sol-gel technique and their
sizes were measured using XRD. We have compared the XRD pattern of Ni doped BaTiO3 with standard BaTiO3
sample which was derived by heating the pellets of the samples at 750o
C for two hours in air. The obtained
results contained the same peak position of BaTiO3 along with peaks of nickel. The peaks were found to be
analogous to the tetragonal structure of the BaTiO3. Fig.2 shows an SEM micrograph of 0.5 mole% Ni+2
doped
BaTiO3. The polymer PVA easily forms the networking with the reinforcing constituents and also adjusts the
sizes of the grains. It serves as a better surfactant to encapsulate the cationic species in the available –OH
functional and long chain coiling with hydrogen bond during the reaction.
3.2 Characterization of the Composite materials
Generally, the chemically dissimilar nature of the soft and hard segments in polyurethane tends to produce
incompatible structures and thus separate the product into different phases during its formation. The dissimilarity
arises from the use of two different reactants and present in the functional group in the reactant molecules. Their
compatibility can be improved by varying the equivalent ratio of the isocyanate (-NCO) group to the hydroxyl (-
OH) group in polyurethane. Fig.3 shows a representative SEM morphology of the modified PU/PEMA
composite with uniform distribution of the ferroelectric materials. A good contrast between two distinguished
phases could be obtained. The IPN matrix appears white and ferroelectric materials appear black. It illustrates
that a good dispersion of toughening particles is achieved at the time of polymerization and addition of second
phase particles. The filler nano particles of ferroelectric materials are distributed in a relatively uniform fashion
and the particles are almost spherical in shape with irregular boundaries. The filler particles are seen to be clearly
embedded in the polymer matrix. These particles maintain the connectivity of the polymer matrix and reinforce
the constituents. The ceramic-polymer composites are made up of an active ceramic phase embedded in a
passive polymer phase. The properties of the composite depend on the connectivity of the phases, volume
percent of ceramic, and the spatial distribution of the active phase in passive phase.
3.3 Effect of the hard/soft phase of polymer segment ratio on the mechanical testing
Engineering materials such as polymer, rubber and metals which are elevated to high temperatures
show plastic deformation when subjected to stress or strain. Such flow is accompanied by the dissipation of
energy due to some internal loss mechanism. Bond breakage, bond formation reaction, dislocation and the
formation of the substructure in metals account for the internal loss mechanism in the material. Materials of this
type are known as visco-elastic in response.
Tensile testing with different ratios of soft and hard phase in IPN matrix was performed to determine
the bulk mechanical properties of polymer nano-composites. The main factors such as molecular weight,
tacticity, and processing history with different contents of the reinforcing constituents, impact mechanical
properties of the polymer nano-composite; pure polymer reference systems were tested to ensure more direct
comparison with nano-composites. In order to test the composites mechanically, we had to prepare suitable
samples from the bulk composite materials. This kind of measurement requires the samples to be of “dog bone”
shape. Hydraulic wedge grips were used to secure both ends of the dog bone. Then the universal testing system
(MECH C.S. /UTE) was used to experimentally apply increasing load in order to maintain a rate of stretching of
0.25 inches per minute. The sample was stretched until it reached the fracture point, making this a destructive

Vol.3 No.9, 2013
68
measurement. Tensile testing data was plotted using stress versus strain curves at different operating
temperatures, the examples of which are shown in Figure 2. Elastic modulus is defined as the slope of the linear
portion of the stress/strain curve. Fig 2 (a) shows the stress strain diagram of the polymer matrix of different soft
to hard phase ratio at room temperature. In the polymer matrix from 80:20 to 20:80 the soft phase of the
polymer decreases while the hard phase of the polymer increases. The fracture stress or UTS increases
continuously as the amount of hard phase in the matrix increases. The nature of the polymer changes with
change in percentage of the hard phase content in the matrix. 20:80 polymers are brittle and 80:20 polymers are
ductile.
3.4 Mechanical properties of Nano-Ba(Ti1-zXz)O3 doped in polymers alloys at the different
temperatures.
The polymer matrix provides many advantages such as easy processing, low cost and resistance to corrosion. In
many circumstances, the polymeric matrix has been the major constituent contributing to degradation or changes
in durability of PMCS. In applications when the matrix material on exposure to environment results in alteration
of the properties of the matrix or mechanical loads that act over long time periods, the visco-elastic nature of the
matrix becomes a dominant factor in the composite performance. Fig.4-6 (a-c) shows the stress-strain curves of
the polymer nanocomposite at different temperatures. With increase in the percentage of the hard phase in the
matrix along with reinforcing constituents, the tensile strength increases with decrease in the size of the
reinforcing constituents in the matrix. With increase in temperature, the tensile strength decreases as shown in
Fig.7. Fig.8 shows the variation of the stress with strain at room temperature with different sizes of the
reinforcing constituents. A smaller size of the reinforcing constituents shows higher tensile strength at the room
temperature.
3.5Impacts of variable amounts of reinforcing constituents in polymers alloys at room
temperatures.
Fig. 9 represents the effect of filler (BaTiO3) loading on tensile strength. From this figure, it is observed that the
tensile strength decreases continuously with the increase in filler concentration. The decrease in both tensile
strength and % E.B. with filler loading are due to non-reinforcing nature of Ni-doped BaTiO3 in IPN matrix.
Maximum strength was found when the amount of filler constituents in the IPN matrix was low. During this
study, the ratio of hard and soft phase in the IPN matrix was kept constant.
Conclusion
Results suggest that the size of the Ba(Ti1-zXz)O3,temperature and ratio of hard phase and soft phase are
parameters influencing the rheological properties of the material. The tensile strength of the composite material
is proportional to the percentage of hard-phase content and inversely proportional to the size of the reinforcing
constituents and temperature. Therefore, the material which has hard phase/soft phase ratio as 90:10 with 48nm
sized Ba(Ti1-zXz)O3 particles doped in the IPN matrix when maintained at room temperature showed the highest
strength.
Reference
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Clanrendon Press, Oxford.
2. Kaiser C. J., (1995). The capacitor handbook. Olathe: CJ Publishing;. p 133.
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G, (2008). Solid state double layer capacitor based on a polyether polymer electrolyte blend and
nanostructured carbon black electrode composites. J. Power Sources, 177, 652 659.
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239, ACS Books, Washington, DC.
6. Miyata T. (2002). Supramolecular Design for Biological Applications, CRC Press.
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517-520
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Polyurethane-Polyepoxide Interpenetrating Polymer Networks [J]. J Appl. Polym. Sci, (18) : 689-693.

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10. Hsieh K. H., Chiang Y. C., Chern Y. C., (1991). Interpenetrating Polymer Network of Polyurethane and
Epoxy I Mechanical Behavior [J]. Angew Makromol Chem, 1991,193: 89-98.
11. Herbert J. M., (1985). Ceramic Dielectrics and Capacitors (Gordon and Breach,Philadelphia,).
12. Chatterjee T, Krishnamoorti R., (2007). Dynamic consequences of the fractal network of nanotube-poly
(ethylene oxide) nanocomposites. Phys. Rev. E, 75, 050403.13
13. Furtado C. A, de Souza P. P., Silva G. G., Matencio T., Pernaut J. M., (2001). Electrochemical behavior of
polyurethane ether electrolytes/carbon black composites and application to double layer capacitor.
Electrochim. Acta (46), 1629 1634.
14. dos Santos A. S., Leite T. D. N., Furtado C. A., Welter C., Pardini L. C., Silva G. G., (2008) . Morphology,
thermal expansion, and electrical conductivity of multi-walled carbon nanotube/epoxy composites. J. Appl.
Polym. Sci.( 108), 979- 986.
O
N
H3C
CH2
CH3
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O +
O CH2
H
CH
CH3
O H
n
O
N
H3C
CH2
CH3
H
N
HN
H3C
CH2
CH3
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O
O CH2 CH
CH3
O
O
C
O
n
+
O
N
H3C
CH2
N
O
3
70oC
CH3
PU-prepolymer(1)
Scheme-1

Vol.3 No.9, 2013
70
O
N
H3C
CH2
CH3
N
O +
70o
C
2
HN
H3C
CH2
CH3
N
O
OH
O H
m
T-12
OH
O
O
m
O
N
H3C
CH2
CH3
N
O +
HO
O
O
O
O
OH
3
+
HN
H3C
CH2
CH3
NH
HO
O
O
O
O
O
O
3
O
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O C
mO
HO
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O
O
O
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O
3
NH
CH3
CH2
CH3
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MDI PTMG
Dihydroxy tetraethylene glycol dimethacrylate
(DTGM)
DHPU prepolymer
Scheme-2
O
N
H3C
CH2
CH3
N
O
+ PU-prepolymer + DHPU
1,4BD(HO-OH)
TMP
70o
C
T-12
DMF
Free MDI
DHPU/PU IPN polymer matrix
IPN-based nano compsoite of ferroeletric materials
In liquid phase mixing
Scheme-3
Figure.1 Synthetic procedure for the preparation of polymer composite along with
preparation of the matrix

Vol.3 No.9, 2013
71
Fig.2 SEM image of Ni+2
doped BaTiO3
Fig.3 SEM image of Ni+2
doped BaTiO3dispersed in IPN polymer matrix

Vol.3 No.9, 2013
72
0 5 10 15 20 25
0
2
4
6
8
10
12
Stress(MPa)
Strain(%)
80:20:00
65:35:00
50:50:00
35:65:00
20:80:00
0 5 10 15 20 25
0
2
4
6
8
10
Stress(MPa)
Strain(%)
80:20:00
65:35:00
50:50:00
35:65:00
20:80:00
(a)25o
C (b) 75o
C
0 5 10 15 20 25
0
2
4
6
8
10
12
Stress(MPa)
Strain(%)
80:20:00
65:35:00
50:50:00
35:65:00
20:80:00
(a) 130o
C
Fig.2(a-c) Stress-Strain diagram of different types of IPN matrix at the different
temperature

Vol.3 No.9, 2013
73
8 12 16 20 24 28
3
4
5
6
7
8
9
10
11
30%
25%
20% 15%
10%
UTS(MPa)
Strain
130
o
C
75
25
Fig.3 (a-c) Variation of the UTS with strain at the different temperature with the
variation of the hard phase

Vol.3 No.9, 2013
74
0 5 10 15 20 25
0
2
4
6
8
10
12
Stress(MPa)
Strain(%)
90:10:00
85:15:00
80:20:00
75:25:00
70:30:00
0 5 10 15 20 25
0
2
4
6
8
10
12
Stress(MPa)
Strain(%)
90:10:00
85:15:00
80:20:00
75:25:00
70:30:00
(a) 25o
C (b) 75o
C
0 5 10 15 20 25
0
2
4
6
8
10
Stress(MPa)
Strain (%)
90:10:00
85:15:00
80:20:00
75:25:00
70:30:00
(C) 1300
C
Fig.4 (a-c) Stress-Strain diagram of 95 nm sizes of Ba (Ti1-zXz)O3 doped in IPN polymer
matrix at different temperatures

Vol.3 No.9, 2013
75
0 5 10 15 20 25
0
2
4
6
8
10
12
Stress(MPa)
Strain(%)
90:10:00
85:15:00
80:20:00
75:25:00
70:30:10
0 5 10 15 20 25
0
2
4
6
8
10
12
Stress(MPa)
Strain(%)
90:10:00
85:15:00
80:20:00
75:25:00
70:30:00
(a)25o
C (b) 75o
C
0 5 10 15 20 25
0
2
4
6
8
10
12
Stress(MPa)
Strain(%)
90:10:00
85:15:00
80:20:00
75:25:00
70:30:00
(c) 130o
C
Fig.5(a-c) Stress-Strain diagram of 68 nm sizes of Ba(Ti1-zXz)O3 doped in IPN polymer
matrix at different temperatures

Vol.3 No.9, 2013
76
0 5 10 15 20 25
0
2
4
6
8
10
12
Stress(MPa)
Strain(%)
90:10:00
85:15:00
80:20:00
75:25:00
70:30:00
0 5 10 15 20 25
0
2
4
6
8
10
12
Stress(MPa)
Strain(%)
90:10:00
85:15:00
80:20:00
75:25:00
70:30:00
(a) 25o
C (b) 70o
C
0 5 10 15 20 25
0
2
4
6
8
10
12
Stress(MPa)
Strain(%)
90:10:00
85:15:00
80:20:00
75:25:00
70:30:00
(c)130o
C
Fig.6(a-c)Stress-Strain diagram of 48 nm sized Ba(Ti1-zXz)O3 particles doped in IPN
polymer matrix at different temperatures

Vol.3 No.9, 2013
77
5 10 15 20 25
2
4
6
8
10
15%
20%
30%
25%
10%
UTS(MPa)
Strain(%)
25
o
C
75
130
Fig.7 Variation of the UTS with strain of 95 nm sized particles of Ba (Ti1-zXz) O3 doped
in IPN polymer matrix at different temperatures
0 4 8 12 16 20 24
0
1
2
3
4
5
6
Stress(MPa)
Strain(%)
95nm
68nm
48nm
Fig.8 Variation of Stress with strain of different sizes of Ba (Ti1-zXz) O3 particles doped in
IPN polymer matrix at room temperature

Vol.3 No.9, 2013
78
2 4 6 8 10 12 14 16
2.0
2.4
2.8
3.2
3.6
4.0
4.4
4.8
5.2
5.6
TensileStrength(MPa)
Amount of the filler in the matrix(%)
95nm
68nm
48nm
Fig.9 Variation of the Stress with strain of different sizes of Ba1-xNixTiO3doped in IPN’s
polymer matrix at room temperature

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